Thioacetamide → Methyl 2-methyl-1,3-thiazole-5-carboxylate
反応式
[CH:1]([CH:3](Cl)[C:4]([O:6][CH3:7])=[O:5])=O.[C:9]([NH2:12])(=[S:11])[CH3:10]>O>[CH3:10][C:9]1[S:11][C:3]([C:4]([O:6][CH3:7])=[O:5])=[CH:1][N:12]=1参加物
4
実験手順
2.0 g (14.6 mmol) methyl formylchloroacetate (A. Gangjee, A. Vidwans, E. Elzein, et. Al. J. Med. Chem. 2001, 44, 1993-2003), and 1.6 g (21.3 mmol) thioacetamide were dissolved in 10 ml water, heated, and reacted at 95° C. for 5 hr. The reaction product was extracted with ethyl acetate for 3 times, the ethyl acetate phases were combined, washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate, filtered, concentrated, and separated by a column chromatography to obtain 1.0 g methyl 2-methylthiazol-5-carboxylate (yield 43%), 1H NMR (CDCl3) 2.76 (3H, s), 3.89 (3H, s), 8.25 (1H, s).
後処理
- temperatureheated
- customreacted at 95° C. for 5 hr
- extractionThe reaction product was extracted with ethyl acetate for 3 times
- washwashed with a saturated sodium chloride solution
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customseparated by a column chromatography
出典と根拠
- ORDレコード
- ord-aa214b6c6d174096a9f64c8cd4bbda1f
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08168642B2
反応ノート
読み込み中…